CN107008260A - A kind of preparation method of low paraffin dehydrogenation catalyst - Google Patents

A kind of preparation method of low paraffin dehydrogenation catalyst Download PDF

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Publication number
CN107008260A
CN107008260A CN201710403821.3A CN201710403821A CN107008260A CN 107008260 A CN107008260 A CN 107008260A CN 201710403821 A CN201710403821 A CN 201710403821A CN 107008260 A CN107008260 A CN 107008260A
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CN
China
Prior art keywords
preparation
dehydrogenation catalyst
paraffin dehydrogenation
alumina
low paraffin
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Pending
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CN201710403821.3A
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Chinese (zh)
Inventor
姚斐
陈广忠
郝新宇
饭田逸夫
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High Chemical (jiangsu) Chemical New Material Co Ltd
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High Chemical (jiangsu) Chemical New Material Co Ltd
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Priority to CN201710403821.3A priority Critical patent/CN107008260A/en
Publication of CN107008260A publication Critical patent/CN107008260A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/002Mixed oxides other than spinels, e.g. perovskite
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/54Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/56Platinum group metals
    • B01J23/62Platinum group metals with gallium, indium, thallium, germanium, tin or lead
    • B01J23/622Platinum group metals with gallium, indium, thallium, germanium, tin or lead with germanium, tin or lead
    • B01J23/626Platinum group metals with gallium, indium, thallium, germanium, tin or lead with germanium, tin or lead with tin
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/60Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J35/61Surface area
    • B01J35/61310-100 m2/g
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/60Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J35/61Surface area
    • B01J35/615100-500 m2/g
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/60Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J35/64Pore diameter
    • B01J35/6472-50 nm
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C5/00Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms
    • C07C5/32Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by dehydrogenation with formation of free hydrogen
    • C07C5/327Formation of non-aromatic carbon-to-carbon double bonds only
    • C07C5/333Catalytic processes
    • C07C5/3335Catalytic processes with metals
    • C07C5/3337Catalytic processes with metals of the platinum group
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2523/00Constitutive chemical elements of heterogeneous catalysts
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/52Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Catalysts (AREA)

Abstract

The present invention provides a kind of preparation method of low paraffin dehydrogenation catalyst, comprises the following steps:S1, preparation θ alumina supports;S2, carrying active ingredients and auxiliary agent are in θ alumina supports.The present invention provides a kind of method for preparing low paraffin dehydrogenation catalyst by θ alumina supports, and to possess carbon distribution few, the characteristics of long lifespan.

Description

A kind of preparation method of low paraffin dehydrogenation catalyst
Technical field
The invention belongs to field of catalyst preparation, it is related to a kind of method of low paraffin dehydrogenation catalyst, particularly one kind Method for preparing catalyst for the anti-carbon of preparing propylene by dehydrogenating propane.
Background technology
Propylene is a kind of important basic organic chemical raw material, and traditional production technology by petroleum cracking route is difficult to Growing propylene demand is met, therefore, is existed in recent years using the technology of abundant and cheap Trends In Preparation of Propene By Catalytic Dehydrogenation of Propane The country is developed rapidly.
The key of dehydrogenating propane technology is the exploitation of catalyst, has applied for Patents by Duo Jia research units both at home and abroad. Traditional makees carrier for preparing propylene by dehydrogenating propane reaction, such as CN102049267A, CN102698750A with gama-alumina;Cause This in recent years many patents propose with molecular sieve as carrier, such as CN106362791A, CN105148979A.
Aluminum oxide is catalyst common carrier, different with sintering temperature according to presoma species, can obtain different crystal forms. Gama-alumina is big due to surface area, and aperture is small and abundant, beneficial to the scattered of active metal, is the crystal formation commonly used in catalyst. Sintering temperature is conventional during the preparation of gama-alumina 300~700 DEG C, in higher temperature, are calcined, aperture at such as 800~1000 DEG C Disappear, specific surface area is reduced, transformation of crystal is θ-aluminum oxide, and using common dipping method, active metal is difficult to disperse, therefore The introducing of dispersion aids becomes extremely important.
Because dehydrogenating propane is strong endothermic reaction, reaction is carried out at high temperature, the easy coking of catalyst, in existing patent, Either gama-alumina or molecular sieve, specific surface area it is big (>150m2/ g), containing more micropore, carbon distribution holds in production Duct is easily blocked, causes the inactivation of catalyst fast, needs frequent regeneration.
The content of the invention
It is an object of the invention to provide a kind of preparation method of low paraffin dehydrogenation catalyst, solve in above-mentioned technical problem One or more.
The present invention provides a kind of preparation method of low paraffin dehydrogenation catalyst, comprises the following steps:
S1, preparation θ-alumina support;
S2, carrying active ingredients and auxiliary agent are in θ-alumina support.
The present invention provides a kind of method that low paraffin dehydrogenation catalyst is prepared by θ-alumina support, and θ-aluminum oxide has Following characteristics:Specific surface area 50-150m2/g;Aperture > 20nm;Intensity > 50N/;Therefore possess that carbon distribution is few, the spy of long lifespan Point.
In some embodiments, the step of preparing θ-alumina support in S1, is mediated using Alumina gel and shaping assistant Uniformly, extrude, granulate, drying, 900 DEG C~1050 DEG C roastings obtain θ-alumina support in 3~10 hours.
In some embodiments, the solute raw material of Alumina gel is at least one of boehmite, both boehmites, The peptizing agent of Alumina gel is inorganic acid or organic acid.
In some embodiments, the solute raw material of Alumina gel also includes aluminium hydroxide.
In some embodiments, shaping assistant is sesbania powder, cellulose, polyethylene glycol, the weight of shaping assistant for θ- The 4~8% of carrying alumina body weight.
In some embodiments, active component is Pt, active component weight for θ-carrying alumina body weight 0.1~ 0.5%;
The step of carrying active ingredients is:θ-alumina support is immersed in the aqueous solution of potassium chloroplatinate, abundant saturation Afterwards, take out, dry.
In some embodiments, S3,600 DEG C of roastings in addition to after S2.
In some embodiments, auxiliary agent includes Sn in S2, and Sn contents are the 0.1~2% of θ-carrying alumina body weight;
Load Sn auxiliary agents the step of be:θ-aluminum oxide is immersed in 50%SnCl4Ethanol solution in, after abundant saturation, Take out, dry.
In some embodiments, auxiliary agent also includes alkali metal or alkaline-earth metal in S2, and alkali metal or alkaline-earth metal contain Measure as the 0.1~1% of θ-carrying alumina body weight;
The step of carrying alkali metal or base earth metal promoter is:θ-aluminum oxide is immersed in magnesium chloride, sodium chloride, potassium chloride Solution in, after abundant saturation, take out, dry.
Embodiment
The present invention provides a kind of preparation method of low paraffin dehydrogenation catalyst, comprises the following steps:
S1, preparation θ-alumina support;
S2, carrying active ingredients and auxiliary agent are in θ-alumina support.
The present invention provides a kind of method that low paraffin dehydrogenation catalyst is prepared by θ-alumina support, and θ-aluminum oxide has Following characteristics:Specific surface area 50-150m2/g;Aperture > 20nm;Intensity > 50N/;Therefore possess that carbon distribution is few, the spy of long lifespan Point.
In a kind of various embodiments of the preparation method for low paraffin dehydrogenation catalyst that the present invention is provided, prepared in S1 The step of θ-alumina support, it is preferable that
Mediated uniformly using Alumina gel and shaping additive, extrusion, granulation, dry, 900 DEG C~1050 DEG C roastings 3~10 are small When obtain θ-alumina support.
In a kind of various embodiments of the preparation method for low paraffin dehydrogenation catalyst that the present invention is provided, prepared in S1 The step of θ-alumina support, it is preferable that
The solute raw material of Alumina gel is at least one of boehmite, both boehmites, and the peptizing agent of Alumina gel is Inorganic acid or organic acid.
In a kind of various embodiments of the preparation method for low paraffin dehydrogenation catalyst that the present invention is provided, prepared in S1 The step of θ-alumina support, it is preferable that
The solute raw material of Alumina gel also includes aluminium hydroxide.
In a kind of various embodiments of the preparation method for low paraffin dehydrogenation catalyst that the present invention is provided, prepared in S1 The step of θ-alumina support, it is preferable that
Shaping assistant is sesbania powder, cellulose, polyethylene glycol, and the weight of shaping assistant is the 4 of θ-carrying alumina body weight ~8%.
It is excellent in S2 in a kind of various embodiments of the preparation method for low paraffin dehydrogenation catalyst that the present invention is provided Choosing,
Active component is Pt, and active component weight is the 0.1~0.5% of θ-carrying alumina body weight;
The step of carrying active ingredients is:θ-alumina support is immersed in the aqueous solution of potassium chloroplatinate, abundant saturation Afterwards, take out, dry.
In a kind of various embodiments of the preparation method for low paraffin dehydrogenation catalyst that the present invention is provided, it is preferable that also Including the S3 after S2,600 DEG C of roastings.
In a kind of various embodiments of the preparation method for low paraffin dehydrogenation catalyst that the present invention is provided, it is preferable that S2 Middle auxiliary agent includes Sn, and Sn contents are the 0.1~2% of θ-carrying alumina body weight;
Load Sn auxiliary agents the step of be:θ-aluminum oxide is immersed in 50%SnCl4Ethanol solution in, after abundant saturation, Take out, dry.
In a kind of various embodiments of the preparation method for low paraffin dehydrogenation catalyst that the present invention is provided, it is preferable that S2 Middle auxiliary agent also includes alkali metal or alkaline-earth metal, the content of alkali metal or alkaline-earth metal for θ-carrying alumina body weight 0.1~ 1%;
The step of carrying alkali metal or base earth metal promoter is:θ-aluminum oxide is immersed in magnesium chloride, sodium chloride, potassium chloride Solution in, after abundant saturation, take out, dry.
With reference to embodiment, the present invention is further detailed explanation.
Embodiment 1:
S1, preparation θ-alumina support;
By boehmite, 5% nitric acid of boehmite parts by weight, boehmite parts by weight 3% Sesbania powder, is well mixed, and the kneading that adds water is agglomerating, and pelletizing is extruded with banded extruder, and disk is shaped to particle diameter 2mm ball;At 120 DEG C Drying 12 hours, 1000 DEG C are calcined 3~10 hours, and carrier is made;The mass fraction of above-mentioned nitric acid is 65%.
S2, carrying active ingredients and auxiliary agent are in θ-alumina support;
Carrier impregnation is in 50%SnCl4Ethanol solution in, after abundant saturation, take out, under 80 DEG C of moving airs dry 8 Hour, Sn contents are 1.0% in carrier;
Again by carrier impregnation in the aqueous solution of potassium chloroplatinate and potassium chloride, after abundant saturation, take out, 120 DEG C of dryings 8 are small When, Pt contents are 0.5% in sample, and potassium content is 0.8%.
S3,600 DEG C be calcined 4 hours, obtain supporting Pt-Sn-K propane dehydrogenation catalyst finished products.
Embodiment 2:
S1 carrier impregnation is in magnesium chloride solution in S2, Example 1, after abundant saturation, 105 DEG C of dryings 4 hours, 800 DEG C are calcined 4 hours, and magnesium 1.0% is contained in carrier;
Again by carrier impregnation in SnCl4In the mixed solution of chloroplatinic acid, after abundant saturation, take out, 120 DEG C of dryings 8 are small When, Pt contents are that 0.3%, Sn contents are 0.3%;
S3, by carrier in 600 DEG C be calcined 4 hours, obtain Pt-Sn-Mg propane dehydrogenation catalyst finished products.
Embodiment 3:
S1 carrier impregnation is in SnCl in S2, Example 14Ethanol solution in, after abundant saturation, take out, at 80 DEG C Dried 4 hours under moving air, Sn contents are 0.5% in carrier;
Carrier impregnation is in platinum acid chloride solution, after abundant saturation, takes out, and 250 DEG C are calcined 4 hours, and Pt contents are in sample 0.5%;
Again by carrier impregnation in sodium chloride solution, after abundant saturation, take out, 120 DEG C of dryings 4 hours, sodium contains in sample Measure as 0.8%;
S3,600 DEG C of carrier are calcined 4 hours, obtain supporting Pt-Sn-Na propane dehydrogenation catalyst finished products.
Above-described is only some embodiments of the present invention.For the person of ordinary skill of the art, not On the premise of departing from the invention design, various modifications and improvements can be made, these belong to the protection model of the present invention Enclose.

Claims (9)

1. a kind of preparation method of low paraffin dehydrogenation catalyst, it is characterised in that comprise the following steps:
S1, preparation θ-alumina support;
S2, carrying active ingredients and auxiliary agent are in the θ-alumina support.
2. the preparation method of a kind of low paraffin dehydrogenation catalyst according to claim 1, it is characterised in that prepared in S1 The step of θ-alumina support, mediated using Alumina gel and shaping assistant it is uniform, extrusion, granulation, dry, 900 DEG C~1050 DEG C Roasting obtains θ-alumina support in 3~10 hours.
3. the preparation method of a kind of low paraffin dehydrogenation catalyst according to claim 2, it is characterised in that the aluminium is molten The solute raw material of glue is at least one of boehmite, both boehmites, the peptizing agent of the Alumina gel for inorganic acid or Organic acid.
4. the preparation method of a kind of low paraffin dehydrogenation catalyst according to claim 3, it is characterised in that the aluminium is molten The solute raw material of glue also includes aluminium hydroxide.
5. a kind of preparation method of low paraffin dehydrogenation catalyst according to claim 2, it is characterised in that the shaping Auxiliary agent is sesbania powder, cellulose, polyethylene glycol, the weight of the shaping assistant for the θ-carrying alumina body weight 4~ 8%.
6. a kind of preparation method of low paraffin dehydrogenation catalyst according to claim 1, it is characterised in that the activity Composition is Pt, and active component weight is the 0.1~0.5% of the θ-carrying alumina body weight;
The step of carrying active ingredients is:θ-alumina support is immersed in the aqueous solution of potassium chloroplatinate, abundant saturation Afterwards, take out, dry.
7. the preparation method of a kind of low paraffin dehydrogenation catalyst according to claim 1, it is characterised in that also including S2 S3 afterwards, 600 DEG C of roastings.
8. the preparation method of a kind of low paraffin dehydrogenation catalyst according to claim 1, it is characterised in that described in S2 Auxiliary agent includes Sn, and Sn contents are the 0.1~2% of the θ-carrying alumina body weight;
The step of loading the Sn auxiliary agents be:θ-the aluminum oxide is immersed in 50%SnCl4Ethanol solution in, abundant saturation Afterwards, take out, dry.
9. the preparation method of a kind of low paraffin dehydrogenation catalyst according to claim 8, it is characterised in that described in S2 Auxiliary agent also includes alkali metal or alkaline-earth metal, and the content of the alkali metal or alkaline-earth metal is the θ-carrying alumina body weight 0.1~1%;
The step of loading the alkali metal or base earth metal promoter be:θ-the aluminum oxide is immersed in magnesium chloride, sodium chloride, chlorine In the solution for changing potassium, after abundant saturation, take out, dry.
CN201710403821.3A 2017-06-01 2017-06-01 A kind of preparation method of low paraffin dehydrogenation catalyst Pending CN107008260A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111632627A (en) * 2020-05-18 2020-09-08 上海国惠环保科技集团有限公司 Preparation method of structural auxiliary for molding
CN115487851A (en) * 2021-06-18 2022-12-20 中国石油化工股份有限公司 Spherical dehydrogenation catalyst, preparation method thereof and application of spherical dehydrogenation catalyst in reaction for preparing isobutene through isobutane dehydrogenation
CN115487795A (en) * 2021-06-18 2022-12-20 中国石油化工股份有限公司 Spherical alumina carrier and preparation method thereof, dehydrogenation catalyst and application
CN115487852A (en) * 2021-06-18 2022-12-20 中国石油化工股份有限公司 Spherical non-noble metal catalyst, preparation method thereof and application thereof in preparation of propylene by propane dehydrogenation
CN115487856A (en) * 2021-06-18 2022-12-20 中国石油化工股份有限公司 Spherical esterification catalyst, preparation method thereof and application thereof in acetate synthesis reaction

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CN102730724A (en) * 2012-05-31 2012-10-17 江苏晶晶新材料有限公司 Preparation process for large pore volume and light bulk density activated alumina
CN103480359A (en) * 2013-09-26 2014-01-01 中国海洋石油总公司 Preparation method for light alkane dehydrogenation catalyst with non-uniformly distributed active components
CN105312046A (en) * 2015-11-05 2016-02-10 中国海洋石油总公司 Light alkane dehydrogenation catalyst and method for improving activity and stability thereof

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CN102730724A (en) * 2012-05-31 2012-10-17 江苏晶晶新材料有限公司 Preparation process for large pore volume and light bulk density activated alumina
CN103480359A (en) * 2013-09-26 2014-01-01 中国海洋石油总公司 Preparation method for light alkane dehydrogenation catalyst with non-uniformly distributed active components
CN105312046A (en) * 2015-11-05 2016-02-10 中国海洋石油总公司 Light alkane dehydrogenation catalyst and method for improving activity and stability thereof

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111632627A (en) * 2020-05-18 2020-09-08 上海国惠环保科技集团有限公司 Preparation method of structural auxiliary for molding
CN115487851A (en) * 2021-06-18 2022-12-20 中国石油化工股份有限公司 Spherical dehydrogenation catalyst, preparation method thereof and application of spherical dehydrogenation catalyst in reaction for preparing isobutene through isobutane dehydrogenation
CN115487795A (en) * 2021-06-18 2022-12-20 中国石油化工股份有限公司 Spherical alumina carrier and preparation method thereof, dehydrogenation catalyst and application
CN115487852A (en) * 2021-06-18 2022-12-20 中国石油化工股份有限公司 Spherical non-noble metal catalyst, preparation method thereof and application thereof in preparation of propylene by propane dehydrogenation
CN115487856A (en) * 2021-06-18 2022-12-20 中国石油化工股份有限公司 Spherical esterification catalyst, preparation method thereof and application thereof in acetate synthesis reaction
CN115487852B (en) * 2021-06-18 2024-06-04 中国石油化工股份有限公司 Spherical non-noble metal catalyst, preparation method thereof and application thereof in propylene preparation by propane dehydrogenation

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Application publication date: 20170804